反应详情

Tetrasodium diphosphate decahydrate (1.5 g, 3.4 mmol) was dissolved in water (34 ml) and the solution was applied to a column of dowex in the H+ form. The column was eluted with water. The eluent dropped directly into a cooled (ice bath) and stirred solution of tri-n-butylamine (1.6 ml, 6.8 mmol) in EtOH (14 ml). The column was washed until the pH of the eluent increased to 6. The aq. ethanol solution was evaporated to dryness and then co-evaporated twice with ethanol and twice with anhydrous DMF. The residue was dissolved in DMF (6.7 ml). The pale yellow solution was stored over 4 Å molecular sieves.

1. washThe column was eluted with water
2. additionThe eluent dropped directly into
3. temperaturea cooled (ice bath)
4. washThe column was washed until the pH of the eluent
5. temperatureincreased to 6
6. customThe aq. ethanol solution was evaporated to dryness
7. dissolutionThe residue was dissolved in DMF (6.7 ml)